CN111896527B - Multi-target ablation device for overcoming spatial position effect in laser micro-area in-situ test - Google Patents
Multi-target ablation device for overcoming spatial position effect in laser micro-area in-situ test Download PDFInfo
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- CN111896527B CN111896527B CN202010766686.0A CN202010766686A CN111896527B CN 111896527 B CN111896527 B CN 111896527B CN 202010766686 A CN202010766686 A CN 202010766686A CN 111896527 B CN111896527 B CN 111896527B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/70—Auxiliary operations or equipment
- B23K26/702—Auxiliary equipment
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0459—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for solid samples
- H01J49/0463—Desorption by laser or particle beam, followed by ionisation as a separate step
Abstract
The invention provides a multi-target ablation device for overcoming the spatial position effect in laser micro-area in-situ test, which comprises a sample table, a laser head and an ablation pool, wherein the ablation pool is fixed under the laser head through a connecting rod, the ablation pool is of a hollow structure, a transparent window for laser to pass through is hermetically arranged at an opening at the top of the ablation pool, an inner cavity of the ablation pool is divided into an inner layer and an outer layer by a spacer ring, the inner layer is an ablation cavity, the outer layer is a vacuum cavity, an air inlet pipe and an air outlet pipe are respectively arranged at two sides of the ablation cavity, and a vacuumizing port is arranged on the side wall of the vacuum cavity and connected with a vacuum generator; the sample platform is arranged on the three-axis displacement platform and is of a double-layer plate structure. The multi-target position denudation device not only has a plurality of target positions, but also is convenient to switch among the target positions, meanwhile, the denudation pool is sealed by utilizing vacuum, and the integral tightness of the denudation pool can be ensured. Most importantly, the multi-target ablation device can overcome the spatial position effect in the laser micro-area in-situ test.
Description
Technical Field
The invention provides a multi-target laser ablation pool, in particular provides an ablation pool capable of overcoming the spatial position effect in laser micro-area in-situ test, and belongs to the field of laser ablation ion light/mass spectrometry.
Background
The laser ablation inductively coupled plasma optical/mass spectrometry technique is one of the most successful and effective techniques for directly performing elemental or isotopic analysis on a solid sample. When the laser ablation inductively coupled plasma light/mass spectrometry is carried out, a sample is usually placed in an ablation cell, analyte aerosol is generated on the surface of the laser ablation sample, and the analyte aerosol is sent into a plasma light/mass spectrometer by carrier gas for detection. In recent years, the laser ablation system and mass spectrometry combined technology has wide application in the fields of geology, environment, biology, materials, jewelry and the like, and especially in the aspect of geology, the LA-ICP-MS has great demand on the basic research of dating of the accessory minerals such as zircon, monazite and the like, and the analysis of trace elements, isotopes and the like. The ablation cell is an indispensable part of a laser ablation system (LA) and has great influence on the analysis capability of the whole system, and the size, the geometric shape, the internal space structure and the like of the ablation cell directly influence the signal stability of element analysis. The traditional ablation pool can generate serious problems of memory effect, element fractionation and the like in the laser ablation process, and finally influences the transmission of aerosol and the accuracy of analysis results.
The interior of the conventional denudation pool is an integral cylindrical or rectangular space with an analysis volume of 100cm 3 -200cm 3 The cleaning time after single-pulse ablation can be as long as 10s, and the analyte aerosol generated by laser ablation repeatedly rotates in the ablation pool, so that the surfaces of other samples are easily polluted. And the different positions of the samples in the single large denudation pool can generate inconsistent fractionation effect, thereby influencing the accuracy of the result. The cleaning time can be effectively reduced by reducing the volume of the denudation pool, but the loading capacity of the sample is influenced, the replacement frequency of the sample in the actual analysis process is increased, and the analysis efficiency and stability are influenced. Although the variety of the ablation pools is various, the ablation pools are simple in design and convenient to operate, can obtain smaller position effect and memory effect and are still less suitable for single-volume ablation pools aiming at single mineral targets with fixed sizes. The primary considerations for a denudation cell intended to achieve low position and memory effects are the small volume of the denudation cell and the need to avoid as far as possible the turbulent effects of the gas flow within the denudation cell.
Disclosure of Invention
The invention provides a multi-target ablation device for overcoming the space position effect in a laser micro-area in-situ test, which solves the defects in the background technology. Most importantly, the multi-target ablation device can overcome the spatial position effect in the laser micro-area in-situ test.
The technical scheme adopted for realizing the above purpose of the invention is as follows:
a multi-target ablation device for overcoming spatial position effects in laser micro-area in-situ tests at least comprises a sample table, a laser head and an ablation pool, wherein the laser head is installed on a laser generator, the ablation pool is fixed under the laser head through a connecting rod, the ablation pool is of a hollow structure, the top and the bottom of the ablation pool are both open, a transparent window for laser to pass through is hermetically installed at the opening of the top, an inner cavity of the ablation pool is divided into an inner layer and an outer layer by a spacer ring, the inner layer is an ablation cavity, the outer layer is a vacuum cavity, an air inlet pipe and an air outlet pipe are respectively arranged on two sides of the ablation cavity, the air inlet pipe and the air outlet pipe both pass through the vacuum cavity to be led to the outside, a vacuum pumping port is arranged on the side wall of the vacuum cavity, and the vacuum pumping port is connected with a vacuum generator; the bottom of the denudation pool is integrally flat, and annular sealing rings are arranged on the bottom surface of the pool wall in the denudation pool and the bottom surface of the spacer ring;
the sample table is arranged on the three-axis displacement platform and is of a double-layer plate structure, wherein an upper layer plate and a lower layer plate are connected through a sliding rail and a sliding block, the upper layer plate and the lower layer plate can move horizontally relatively, the lower layer plate is fixed on the three-axis displacement platform through a bolt, and a locking device used for locking the sliding rail and the sliding block is arranged on the lower layer plate; the top surface of the upper plate is a flat and smooth plane, more than one groove for placing target samples of different specifications is distributed on the top surface of the upper plate, and an annular sealing ring is arranged on the inner wall of the groove.
The transparent window adopts 0.2mm thick calcium fluoride glass, and the calcium fluoride glass passes through pressure disk and screw connection to be fixed at ablation pond top opening part.
The aperture of the air inlet hole in the air inlet pipe is 0.5mm, and the aperture of the air outlet hole in the air outlet pipe is 3mm.
The upper plate is provided with three grooves which are respectively used for placing target samples with the diameters of 2.54cm, 1.6cm and 1.0 cm.
The three-axis displacement platform realizes the precise displacement of the sample platform in the X, Y and Z three-axis directions through an operating rod or control software.
The edge of the upper plate is provided with a handle.
Compared with the prior art, the multi-target ablation device for overcoming the spatial position effect in the laser micro-area in-situ test has the following advantages: 1. in order to obtain a lower memory effect and simultaneously avoid a turbulent effect generated by airflow in the denudation pool, the invention adopts a single-pool single-target structure, the air inlet aperture designed in the denudation pool is 0.5mm, and the air outlet aperture is 3mm, so that aerosol particles can quickly pass through the denudation pool to reach ICP for ionization under a higher gas flow rate in the denudation pool, and the memory effect in the denudation pool is greatly reduced. 2. The structure of adopting single cell single target can influence the loading capacity to the sample, increases the change frequency of actual analysis process sample, influences the efficiency and the stability of analysis. In order to solve the problem, the invention creatively provides a multi-target sample platform and a bottom-opening type ablation pool structure, wherein the sample platform is carried on a three-axis displacement platform and can perform precise displacement, and when a target sample needs to be switched, only the position of the sample platform needs to be moved. Meanwhile, in order to ensure the air tightness of the denudation pool and ensure that aerosol cannot leak in the denudation transmission process, the denudation pool is creatively sealed in a vacuum manner, the periphery of the denudation cavity is provided with a vacuum cavity which is connected with a vacuum generator, and the bottom surface of the denudation pool is provided with an annular sealing ring, so that the tightness of the denudation pool is realized, the convenience of multi-target position switching can be considered, and the analysis efficiency cannot be influenced. 3. In the art, even if the same sample target is used, when the laser irradiates different positions on the sample target, the corresponding intensities of the generated signals are different, which is the position effect. In order to solve the problem, the sample stage is arranged on the three-axis displacement platform in a breakthrough manner, so that the sample target can be finely adjusted by utilizing an X axis and a Y axis before denudation, and the sample target is ensured to be always positioned right below the laser lens.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a multi-target ablation apparatus for overcoming spatial position effect in-situ laser micro-area testing provided by the present application;
FIG. 2 is a schematic longitudinal cross-sectional view of an ablation cell;
FIG. 3 is a schematic cross-sectional view of a denudation pool
FIG. 4 is a schematic structural diagram of a sample stage;
FIG. 5 is a bottom view of the upper plate in the sample stage;
FIG. 6 is a view showing the structure of the lower plate of the sample stage;
in the figure: 1-a sample table, 2-a laser head, 3-an ablation tank, 4-a connecting rod, 5-a transparent window, 6-an ablation cavity, 7-a vacuum cavity, 8-an air inlet pipe, 9-an air outlet pipe, 10-a vacuum pumping port, 11-a vacuum generator, 12-a spacer ring, 13-an annular sealing ring, 14-an upper plate, 15-a lower plate, 16-a slide rail, 17-a slide block, 18-a locking device, 19-a groove and 20-a handle.
Detailed Description
The invention is described in detail below with reference to the drawings and specific embodiments.
The overall structure of the multi-target ablation device for overcoming the spatial position effect in the laser micro-area in-situ test is shown in figure 1, and the multi-target ablation device comprises a sample table 1, a laser head 2, an ablation pool 3, a vacuum generator 11 and a three-axis displacement platform (the three-axis displacement platform is not shown in the figure), wherein the laser head 2 is arranged on a laser generator (the laser generator is not shown in the figure), the ablation pool 3 is fixed under the laser head 2 through a connecting rod 4, the sample table 1 is arranged on the three-axis displacement platform, and the sample table 1 is positioned below the ablation pool 3. The three-axis displacement platform realizes the precise displacement of the sample stage in the X, Y and Z three-axis directions through an operating rod or control software.
The structure of the denudation pool is shown in fig. 2 and fig. 3, the denudation pool is of a hollow structure, the top and the bottom of the denudation pool are both open, a transparent window 5 for laser to pass through is hermetically arranged at the opening of the top, the transparent window 5 is made of calcium fluoride glass with the thickness of 0.2mm, and the calcium fluoride glass is fixedly connected with the opening of the top of the denudation pool through a pressing plate and a screw. The inner cavity of the denudation pool is divided into an inner layer and an outer layer by a spacer ring 12, the inner layer is a denudation cavity 6, the outer layer is a vacuum cavity 7, an air inlet pipe 8 and an air outlet pipe 9 are respectively arranged on two sides of the denudation cavity 6, the air inlet pipe 8 and the air outlet pipe 9 penetrate through the vacuum cavity 7 and are communicated with the outside, the aperture of an air inlet hole in the air inlet pipe 8 is 0.5mm, and the aperture of an air outlet hole in the air outlet pipe 9 is 3mm. A vacuumizing port 10 is arranged on the side wall of the vacuum cavity 7 and is connected with a vacuum generator; the bottom of the denudation pool 3 is flat and flat, and the bottom surfaces of the pool wall and the spacer ring in the denudation pool are provided with annular sealing rings 13.
The structure of the sample table is shown in fig. 4, 5 and 6, the sample table is a double-layer plate structure, wherein an upper plate 14 and a lower plate 15 are connected through a slide rail 16 and a slide block 17, the upper plate 14 and the lower plate 15 can relatively translate, the lower plate 15 is fixed on a three-axis displacement platform through bolts, and a locking device 18 for locking the slide rail and the slide block is arranged on the lower plate 15; the top surface of the upper plate 14 is a flat and smooth plane, more than one groove 19 for placing target samples of different specifications is distributed on the top surface of the upper plate 14, and an annular sealing ring is arranged on the inner wall of the groove. The upper plate is provided with three grooves which are respectively used for placing target samples with the diameters of 2.54cm, 1.6cm and 1.0 cm. The edge of the upper plate is provided with a handle 20.
The working principle of the multi-target ablation device for overcoming the spatial position effect in the laser micro-area in-situ test provided by the invention is as follows: firstly, in order to obtain lower memory effect and avoid the turbulent effect generated by airflow in the denudation pool, the invention adopts a structure of single pool and single target. Sample targets with different specifications are respectively fixed in independent grooves, when denudation is carried out, firstly, a Z axis in a three-axis displacement platform moves, a sample table 1 is jacked to be in contact with an denudation pool 3, then, an X axis and a Y axis are finely adjusted, the sample targets are guaranteed to be always located under a laser lens, a vacuum generator is started after positioning, a vacuum cavity 7 in the denudation pool 3 is vacuumized, and under the vacuum action, an annular sealing ring is arranged on the bottom surface of the denudation pool and is tightly attached to the sample table, so that the sealing performance of a single denudation pool is realized. After vacuumizing, laser is started and carrier gas is introduced for denudation, the designed air inlet aperture in the denudation pool is 0.5mm, and the aperture of the air outlet is 3mm, so that aerosol particles can rapidly reach ICP through the denudation pool for ionization at a high gas flow rate in the denudation pool, and the memory effect in the denudation pool is greatly reduced. And after the ablation is finished, closing the laser and stopping introducing the carrier gas, simultaneously stopping the vacuum generator, moving the sample platform 1 downwards along the Z axis to separate the sample platform from the ablation pool 3, then moving the sample platform along the X axis and the Y axis to enable another sample target on the sample platform to be positioned below the ablation pool, and repeating the steps to perform the ablation again. After all sample targets are corroded, when the sample targets need to be replaced on the sample table, the locking device 18 on the sample table 1 can be opened, then the handle on the upper plate 14 is held, the upper plate 14 is pulled out, the sample targets can be conveniently replaced, and after the replacement is finished, the upper plate is pushed in, and the locking device 18 is locked.
Claims (6)
1. The utility model provides an overcome many targets position of laser micro-district normal position test medium space position effect and degrade device, includes sample platform, laser head and degradation pond at least, and the laser head is installed on laser generator, its characterized in that: the laser ablation device comprises an ablation pool, a laser head, a spacer ring, a vacuum generator, an inner cavity, an outer cavity, a vacuum cavity, an air inlet pipe and an air outlet pipe, wherein the ablation pool is fixed under the laser head through a connecting rod and is of a hollow structure, the top and the bottom of the ablation pool are both open, a transparent window for laser to pass through is hermetically arranged at the opening of the top, an inner cavity of the ablation pool is divided into an inner cavity and an outer cavity by the spacer ring, the inner cavity is an ablation cavity, the outer cavity is the vacuum cavity, the air inlet pipe and the air outlet pipe are respectively arranged on two sides of the ablation cavity, the air inlet pipe and the air outlet pipe both pass through the vacuum cavity to the outside, a vacuumizing port is arranged on the side wall of the vacuum cavity, and the vacuumizing port is connected with the vacuum generator; the bottom of the denudation pool is integrally flat, and annular sealing rings are arranged on the bottom surface of the pool wall in the denudation pool and the bottom surface of the spacer ring;
the sample table is arranged on the three-axis displacement platform and is of a double-layer plate structure, wherein an upper layer plate and a lower layer plate are connected through a sliding rail and a sliding block, the upper layer plate and the lower layer plate can move horizontally relatively, the lower layer plate is fixed on the three-axis displacement platform through a bolt, and a locking device used for locking the sliding rail and the sliding block is arranged on the lower layer plate; the top surface of the upper plate is a flat and smooth plane, more than one groove used for placing target samples of different specifications is distributed on the top surface of the upper plate, and an annular sealing ring is arranged on the inner wall of the groove.
2. The multi-target ablation apparatus for overcoming spatial position effect in laser micro-zone in-situ test according to claim 1, wherein: the transparent window adopts 0.2mm thick calcium fluoride glass, and the calcium fluoride glass passes through pressure disk and screw connection to be fixed at ablation pond top opening part.
3. The multi-target ablation apparatus for overcoming spatial position effect in laser micro-zone in-situ test according to claim 1, wherein: the aperture of the air inlet hole in the air inlet pipe is 0.5mm, and the aperture of the air outlet hole in the air outlet pipe is 3mm.
4. The multi-target ablation apparatus for overcoming spatial position effect in laser micro-zone in-situ test according to claim 1, wherein: the upper plate is provided with three grooves which are respectively used for placing target samples with the diameters of 2.54cm, 1.6cm and 1.0 cm.
5. The multi-target ablation apparatus for overcoming spatial position effect in laser micro-zone in-situ test according to claim 1, wherein: the three-axis displacement platform realizes the precise displacement of the sample stage in the X, Y and Z three-axis directions through an operating rod or control software.
6. The multi-target ablation apparatus for overcoming spatial position effect in laser micro-zone in-situ test according to claim 1, wherein: the edge of the upper plate is provided with a handle.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010766686.0A CN111896527B (en) | 2020-08-03 | 2020-08-03 | Multi-target ablation device for overcoming spatial position effect in laser micro-area in-situ test |
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| CN111896527B true CN111896527B (en) | 2023-04-18 |
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| CN113063643B (en) | 2021-03-25 | 2022-02-25 | 中国科学院地质与地球物理研究所 | Double-body-volume freezing ablation pool device for fluid inclusion LA-ICP-MS analysis and ablation method thereof |
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| US9679753B2 (en) * | 2013-03-14 | 2017-06-13 | University Of Massachusetts | Peltier-cooled cryogenic laser ablation cell |
| US9352418B2 (en) * | 2014-01-06 | 2016-05-31 | Teledyne Instruments, Inc. | Laser-ablation-based material analysis system with a power/energy detector |
| CN104075932B (en) * | 2014-06-19 | 2016-08-24 | 袁洪林 | A kind of laser ablation sample room of many target position |
| CN104777155B (en) * | 2015-04-15 | 2017-06-09 | 武汉上谱分析科技有限责任公司 | A kind of rotating channel formula laser ablation pond |
| CN211122659U (en) * | 2019-11-19 | 2020-07-28 | 武汉上谱分析科技有限责任公司 | Small-volume denudation pool with double-size targets |
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